Preparation of RuCl(dppe)Cp

ref: A.G Alonso and L.B Reventos, J.Organomet.Chem.,1998, 338, 249

RuCl(PPh3)2Cp -------------------> RuCl(dppe)Cp
0.277g dppe
100 ml toluene

1. Set up the apparatus. See synthesis of RuCl(PPh3)2. (mass of RuCl(PPh3)2Cp used = 0.5085g)


2. The yellowish solution was let to reflux for about 6 hours
   
3. Next, follow the crystallization step (see previous page)


4. The filtrate volume was reduced to ~20 ml by rotavap


5. n-hexane was added into the solution (in excess)
   
6. Leave the solution which now contains precipitate in freezer for ~20 mins to allow the ppt. to settle down


7. Filter again using vacuum suction


8. The deposited ppt. at the RBF was scratched off using spatula


9. Combine all the products obtained and store in vial

RuCl(dppe)Cp

percentage yield = 46%

Synthesis of RuCl(PPh3)2Cp Part ii

So, yeah..after the vacuum line was succesfully set up..so the excitement beginnnsss...

Here is how the apparatus for the synthesis shall looks like.

Addition of the dissolved RuCl3/EtOH + Cp into the dissolved PPh3/EtOH is by dropwise within about 10 mins period of time.

After about 0ne hour of refluxing, the dark brown color of the solution will lighten to dark red-orange color as shown.

This solution is stored in a freezer at ~-10deg.celc. for an overnight.

iii. Crystallization

Next, filtration of the solution was done using vacuum suction method.



Finally, this is our precius product!!

• Percentage yield = 77%
  
• JMR = 726.3 g/mol


• Analysis = NMR, MS
  
  
  

My 1st synthesis (12 April 2010) - chloro(cyclopentadienyl)bis(triphenyl-phosphine)ruthenium(ii)

Title : Preparation of RuCl(PPh3)2Cp

Procedure

ref: Chloro(η5-Cyclopentadienyl)Bis(Triphenyl-Phosphine) Ruthenium(II): Rucl(PPh3)2(η5-C5H5)Inorganic Syntheses: Reagents for Transition Metal Complex and Organometallic Syntheses, Volume 28 , Pages270 - 272.
M. I. Bruce, C. Hameister, A. G. Swincer, R. C. Wallis, S. D. Ittel
Copyright © 1990 Inorganic Syntheses, Inc

i. Distillation of diCp -> Cp




Make sure!!

• to purge the apparatus with N2 before start distilling
• no leaking
• to attach the water inlet while distilling
• do not use water bath for the distillation, use Silicon oil instead as water can easily evaporated
• the receiver flask must be attached to an ice-containing beaker (to prevent the product to get polymerized back to diCp)
  

ii. synthesis of RuCl(PPh3)2Cp

First of all, set up the vacuum line since the compounds we are dealing with are air-sensitive.

the complete set-up of vacuum line for my bench is shown. Well, bit of messy but as long as you understand the flow, you will get it (i'm still learning).

Make sure!!

• only open the intended use of N2 inlet
• to always check for any leak of the system
• always REMEMBER to remove the N2 cylinder from the system when not in use

Next, we can start to assemble the apparatus for the synthesis. (see next)